CN1293021C - Method for producing metal-ceramic gradient materials - Google Patents

Method for producing metal-ceramic gradient materials Download PDF

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Publication number
CN1293021C
CN1293021C CNB2003101145014A CN200310114501A CN1293021C CN 1293021 C CN1293021 C CN 1293021C CN B2003101145014 A CNB2003101145014 A CN B2003101145014A CN 200310114501 A CN200310114501 A CN 200310114501A CN 1293021 C CN1293021 C CN 1293021C
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metal
ceramic
preparation
mixed
ceramic metal
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CN1629097A (en
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唐竹兴
田贵山
许珂敬
任京成
魏春城
董抒华
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Shandong University of Technology
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Shandong University of Technology
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Abstract

The present invention relates to a preparation method for a ceramic metal gradient material. The method comprises the preparation, the molding and the firing of ceramic metal material slurry. The present invention is characterized in that 136L of stainless steel powder with the granularity of 1 to 100 mum and a ceramic material are mixed with additives according to the weight percentage of the stainless steel powder and the ceramic material to the additives of 80 to 99:1 to 20 after the stainless steel powder is mixed with the ceramic material according to the weight proportion of the stainless steel powder to the ceramic material of 1:1 to 3, and ceramic metal powder is formed; an organic solution is prepared by mixing 1 to 75 wt% of organic substance and 25 to 99 wt% of water, and then, the organic solution is mixed with a dispersing agent according to the weight percentage of 85 to 97:3 to 15; the pH value of the organic solution is regulated to 9 to 10, and a mixed organic solution is prepared; the ceramic metal powder is sufficiently mixed with the mixed organic solution according to the weight percentage of 60 to 99:1 to 30, and suspending ceramic metal material slurry is prepared; after the vacuum treatment of the suspending ceramic metal material slurry is carried out, 0.01 to 0.2 wt% of evocating agent is additionally added, and the suspending ceramic metal material slurry and the evocating agent are stirred; finally, the suspending ceramic metal material slurry and the evocating agent are poured into a mould and solidified under the auxiliary action of fields, and then, the demoulding and the firing of the suspending ceramic metal material slurry and the evocating agent are carried out. In the method of the present invention, a pouring solidification molding technology is used, and the present invention has the advantages of simple technology, convenient operation, short production period, high production efficiency, high production yield, low cost and.

Description

The preparation method of metal-ceramic gradient material
Technical field
The present invention relates to a kind of preparation method of metal-ceramic gradient material, belong to sintering metal fabricating technology field.
Background technology
Prepare the metal-ceramic gradient material both at home and abroad because the restriction of forming method at present, metal-the gradient material that forms is made up of multilayer different content component layer, belong to stepped gradient material, this material is in application process, on aspect, be easy to generate concentrating of stress and thermal stresses, cause layers of material to destroy, destroyed the performance of material itself, poor reliability.Adopt physics, chemical Vapor deposition process (CVD, PVD or PCVD method) even, the gradient material of method preparation such as particle alignment method is the continuous distribution gradient material, because preparation technology's imperfection, only limit to prepare the gradient material of thinner layer (generally being no more than 0.5mm), the actual gradient material layer also only has tens microns, therefore do not satisfy the needs of engineering far away, adopt the requirement of method for preparing gradient material that higher appointed condition is arranged in addition, and the production cost height.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can overcome above-mentioned defective, easy to operate, with short production cycle, the work workload is little, production efficiency height, the rate that manufactures a finished product height, and the preparation method of the metal-ceramic gradient material of good product quality.Its technical scheme is:
Comprise the preparation of metal-ceramic material paste, moulding and burning till, it is characterized in that: it is the 316L stainless steel powder of 1~100 μ m that metallic substance is selected granularity, after stupalith mixes by weight 1: 1~3, again with sintering aid by weight percentage 80~99: 1~20 mixed constitute the sintering metal powder, then with sintering metal powder and mixed organic solvents by weight percentage 60~99: 1~30 thorough mixing make suspension metal-ceramic material paste, the initiator that adds 0.01~0.2wt% after vacuum-treat stirs, inject mould at last 0~100 ℃ of temperature, under the condition of 0.1~3 hour time, at electric field, the booster action of magnetic field and gravity field solidifies down, stripping forming then, base substrate after will drying at last burns till in 1000~1650 ℃ temperature range, wherein stupalith is stabilized with yttrium oxide tetragonal phase zirconium oxide material or aluminum oxide or silicon nitride material, the composition weight percent of sintering aid is: yttrium oxide 30~60, cerium oxide 10~50, magnesium oxide 10~15, magnesium-aluminium spinel 10~15, being prepared as of mixed organic solvents earlier with organism 1~75wt% and the mixed organic solution that gets of water 25~99wt%, again with organic solution with as the polyacrylic acid ammonium solution of dispersion agent by weight percentage 85~97: 3~15 mix after, its pH value is adjusted to 9~11 to get final product, wherein organism is by N, and N-methylene radical acrylamide and acrylamide are formulated.
For achieving the above object, the preparation method of described metal-ceramic gradient material, the organic N that consists of, N-methylene radical acrylamide 1wt%, acrylamide 99wt%.
For achieving the above object, the preparation method of described metal-ceramic gradient material, the concentration of polyacrylic acid ammonium solution are 20~60wt%, and pH value is adjusted agent and adopted 40~60wt% ammoniacal liquor.
For achieving the above object, the preparation method of described metal-ceramic gradient material, it is the ammonium persulfate solution of 1~5wt% that initiator adopts concentration.
For achieving the above object, the preparation method of described metal-ceramic gradient material, the optimum ratio that the metal-ceramic material paste is formed weight is: the sintering metal powder is by 316L stainless steel powder 45~55wt%, stupalith 43~55wt% and sintering aid 2~3wt% form, organic solution is mixed by organism 1~75wt% and water 25~99wt% and is formed, mix after its pH value adjusted to 9~10 at 90~95: 5~10 by weight percentage with dispersion agent again, make mixed organic solvents, sintering metal powder and mixed organic solvents are made suspension metal-ceramic material paste according to the mixed of 70~80wt%:20~30wt% then.
For achieving the above object, the preparation method of described metal-ceramic gradient material, mould adopts non-water-absorbent mould, reaches at water-absorbent moulding stock surface-coated waterproof layer sectional die as metal die, glass mold, mould of plastics.
For achieving the above object, the preparation method of described metal-ceramic gradient material, till metal-ceramic material paste vacuum-treat to vacuum tightness being reached-0.1MPa, not having in the slurry bubble to overflow, adding the initiator final vacuum fully stirs, time was controlled in 3 minutes, slurry is injected mould solidify under the booster action of electric field, magnetic field and gravity field.
The present invention compared with prior art, adopt gel-casting technology to prepare the metal-ceramic slurry, make under the effect in (gravity field, electric field, magnetic field etc.) on the scene that pottery and metallics in the slurry is directed on thickness (gradient) direction to move that (ceramic particle is different with metallic particles direction of motion, or the identical and movement velocity difference of direction of motion), formation to metallic substance, forms the metal-ceramic gradient material of continuous distribution from the stupalith continuous transition.Adopt the metal-ceramic gradient material of this technology preparation, not only realized the continuous transition of gradient layer, and the thickness of gradient layer can reach more than the 3mm, gradient layer material thermal shock resistance (800 ℃~room temperature) reaches and does not occur obvious crackle more than 20 times.This preparation method is easy to operate, and is with short production cycle, and the work workload is little, production efficiency height, the rate that manufactures a finished product height.
Embodiment
Embodiment 1:
Metallic substance adopts the 316L stainless steel powder of 40 μ m; It is the stabilized with yttrium oxide tetragonal phase zirconium oxide of 2 μ m that stupalith adopts granularity, and its batching composition and preparation technology are as follows:
Batching:
Consisting of of sintering metal powder: metallic substance 50wt%, stupalith 48wt% and sintering aid 2wt%, wherein sintering aid consists of yttrium oxide 40wt%, cerium oxide 30wt%, magnesium oxide 15wt% and magnesium-aluminium spinel 15wt%;
Consisting of of organic solution: organism 5wt%, water 95wt%, the wherein organic N that consists of, N-methylene radical acrylamide 2wt%, acrylamide 98wt%;
Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%;
PH value is adjusted agent and is adopted 40wt% ammoniacal liquor;
It is the ammonium persulfate solution of 4wt% that initiator adopts concentration.
Preparation:
With above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to 89: 10: 1 mixed of weight percent, then with the sintering metal powder with add ballstone after mixed organic solvents mixes according to weight percent at 80: 20 and grind, make even suspension metal-ceramic material paste, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having bubble to overflow in the slurry, adding initiator 0.01wt% final vacuum more fully stirs, time was controlled in 3 minutes, slurry is injected mould 90 ℃ of temperature, under the condition of 0.5 hour time, at electric field, the booster action of magnetic field and gravity field solidifies down, the demoulding then; Base substrate after will drying at last burns till in 1580 ℃ temperature range, makes metal-ceramic gradient material of the present invention.
The purity of testing used proportion material is technical pure.
Through check, the technical indicator that makes product is: mean compressive strength 1000MPa.; Thermal shock resistance (room temperature~800 ℃) reaches more than 20 times, and obvious crackle does not appear in the tonsure layer.
Embodiment 2:
Metallic substance adopts the 316L stainless steel powder of 5 μ m; It is the aluminum oxide of 2 μ m that stupalith adopts granularity, and its batching composition and preparation technology are as follows:
Batching:
Consisting of of sintering metal powder: metallic substance 45wt%, stupalith 53wt% and sintering aid 2wt%, wherein sintering aid consists of yttrium oxide 40wt%, cerium oxide 35wt%, magnesium oxide 15wt% and magnesium-aluminium spinel 10wt%;
Consisting of of organic solution: organism 20wt%, water 80wt%, the wherein organic N that consists of, N-methylene radical acrylamide 5wt%, acrylamide 95wt%;
Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%;
PH value is adjusted agent and is adopted 40wt% ammoniacal liquor;
It is the ammonium persulfate solution of 1wt% that initiator adopts concentration.
Preparation:
With above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to 89: 10: 1 mixed of weight percent, then with the sintering metal powder with add ballstone after mixed organic solvents mixes according to weight percent at 80: 20 and grind, make even suspension metal-ceramic material paste, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having bubble to overflow in the slurry, adding initiator 0.06wt% final vacuum more fully stirs, time was controlled in 3 minutes, slurry is injected mould 90 ℃ of temperature, under the condition of 0.5 hour time, at electric field, the booster action of magnetic field and gravity field solidifies down, the demoulding then; Base substrate after will drying at last burns till in 1650 ℃ temperature range, makes metal-ceramic gradient material of the present invention.
The purity of testing used proportion material is technical pure.
Through check, the technical indicator of the product that makes is: mean compressive strength 300MPa.; Thermal shock resistance (room temperature~800 ℃) reaches more than 20 times, and obvious crackle does not appear in the tonsure layer.
Embodiment 3:
Metallic substance adopts the 316L stainless steel powder of 80 μ m; It is the silicon nitride powder of 2 μ m that stupalith adopts granularity, and its batching composition and technology are as follows:
Batching:
Consisting of of sintering metal powder: metallic substance 55wt%, stupalith 43wt% and sintering aid 2wt%, wherein sintering aid consists of yttrium oxide 40wt%, cerium oxide 30wt%, magnesium oxide 15wt% and magnesium-aluminium spinel 15wt%;
Consisting of of organic solution: organism 3wt%, water 95wt%, the wherein organic N that consists of, N-methylene radical acrylamide 10wt%, acrylamide 90wt%;
Dispersion agent adopts the polyacrylic acid ammonium solution, and concentration is 30wt%;
PH value is adjusted agent and is adopted 40wt% ammoniacal liquor;
It is the ammonium persulfate solution of 5wt% that initiator adopts concentration.
Preparation:
With above-mentioned organic solution, dispersion agent, pH value is adjusted agent and is made mixed organic solvents according to 89: 10: 1 mixed of weight percent, then with the sintering metal powder with add ballstone after mixed organic solvents mixes according to weight percent at 80: 20 and grind, make even suspension metal-ceramic material paste, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having bubble to overflow in the slurry, adding initiator 0.1wt% final vacuum more fully stirs, time was controlled in 3 minutes, slurry is injected mould 90 ℃ of temperature, under the condition of 0.5 hour time, at electric field, the booster action of magnetic field and gravity field solidifies down, the demoulding then; Base substrate after will drying at last burns till in 1550 ℃ temperature range, makes metal-ceramic gradient material of the present invention.
The purity of testing used proportion material is technical pure.
Through check, the technical indicator of the product that makes is: mean compressive strength 1000MPa.; Thermal shock resistance (room temperature~800 ℃) reaches more than 20 times, and obvious crackle does not appear in the tonsure layer.

Claims (8)

1, a kind of preparation method of metal-ceramic gradient material, comprise the preparation of metal-ceramic material paste, moulding and burning till, it is characterized in that: it is the 316L stainless steel powder of 1~100 μ m that metallic substance is selected granularity, after stupalith mixes by weight 1: 1~3, again with sintering aid by weight percentage 80~99: 1~20 mixed constitute the sintering metal powder, then with sintering metal powder and mixed organic solvents by weight percentage 60~99: 1~30 thorough mixing make suspension metal-ceramic material paste, the initiator that adds 0.01~0.2wt% after vacuum-treat stirs, inject mould at last 0~100 ℃ of temperature, under the condition of 0.1~3 hour time, at electric field, the booster action of magnetic field and gravity field solidifies down, stripping forming then, base substrate after will drying at last burns till in 1000~1650 ℃ temperature range, wherein stupalith is stabilized with yttrium oxide tetragonal phase zirconium oxide material or aluminum oxide or silicon nitride material, the composition weight percent of sintering aid is: yttrium oxide 30~60, cerium oxide 10~50, magnesium oxide 10~15, magnesium-aluminium spinel 10~15, being prepared as of mixed organic solvents earlier with organism 1~75wt% and the mixed organic solution that gets of water 25~99wt%, again with organic solution with as the polyacrylic acid ammonium solution of dispersion agent by weight percentage 85~97: 3~15 mix after, its pH value is adjusted to 9~11 to get final product, wherein organism is by N, and N-methylene radical acrylamide and acrylamide are formulated.
2, the preparation method of metal-ceramic gradient material as claimed in claim 1 is characterized in that: the organic N of consisting of, N-methylene radical acrylamide 1wt%, acrylamide 99wt%.
3, the preparation method of metal-ceramic gradient material as claimed in claim 1 is characterized in that: the concentration of polyacrylic acid ammonium solution is 20~60wt%, and pH value is adjusted agent and adopted 40~60wt% ammoniacal liquor.
4, the preparation method of metal-ceramic gradient material as claimed in claim 1 is characterized in that: it is the ammonium persulfate solution of 1~5wt% that initiator adopts concentration.
5, the preparation method of metal-ceramic gradient material as claimed in claim 1, it is characterized in that: the optimum ratio that the metal-ceramic material paste is formed weight is: the sintering metal powder is by 316L stainless steel powder 45~55wt%, stupalith 43~55wt% and sintering aid 2~3wt% form, organic solution is mixed by organism 1~75wt% and water 25~99wt% and is formed, mix after its pH value adjusted to 9~10 at 90~95: 5~10 by weight percentage with dispersion agent again, make mixed organic solvents, sintering metal powder and mixed organic solvents are made suspension metal-ceramic material paste according to the mixed of 70~80wt%: 20~30wt% then.
6, the preparation method of metal-ceramic gradient material as claimed in claim 1 is characterized in that: mould adopts non-water-absorbent mould.
7, the preparation method of metal-ceramic gradient material as claimed in claim 6 is characterized in that: non-water-absorbent mould is metal die, glass mold, mould of plastics and at water-absorbent moulding stock surface-coated waterproof layer sectional die.
8, the preparation method of metal-ceramic gradient material as claimed in claim 1, it is characterized in that: till metal-ceramic material paste vacuum-treat to vacuum tightness being reached-0.1MPa, do not have in the slurry bubble to overflow, adding the initiator final vacuum fully stirs, time was controlled in 3 minutes, slurry is injected mould solidify under the booster action of electric field, magnetic field and gravity field.
CNB2003101145014A 2003-12-18 2003-12-18 Method for producing metal-ceramic gradient materials Expired - Fee Related CN1293021C (en)

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1911619B (en) * 2006-09-01 2010-07-28 浙江大学 Preparation method of strong magnetic-weak magnetic gradient material gel injection mould in pulse magnetic field
CN1915626B (en) * 2006-09-01 2010-11-10 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through flow casting molding in pulse magnetism
CN1915625B (en) * 2006-09-01 2010-12-08 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through pressure filtration molding in pulse magnetism
CN101323527B (en) * 2007-06-13 2011-03-02 山东理工大学 Preparation of ceramic thermal protection tube
CN104972130B (en) * 2015-06-28 2017-10-27 中国计量大学 The gel injection moulding preparation of metal and ceramic gradient material in alternating magnetic field
CN113136519B (en) * 2021-04-26 2022-02-18 中建材科创新技术研究院(山东)有限公司 Wear-resistant and corrosion-resistant iron-based composite material and preparation method and application thereof
CN114029490A (en) * 2021-11-29 2022-02-11 深圳艾利佳材料科技有限公司 Three-dimensional metal ceramic gradient material gel casting mould

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10258479A (en) * 1997-03-21 1998-09-29 Honda Motor Co Ltd Manufacture of functionally gradient material
US6248286B1 (en) * 1999-12-03 2001-06-19 Ut-Battelle, Llc Method of making a functionally graded material
CN1438084A (en) * 2003-02-21 2003-08-27 浙江大学 Functional gradient material slip-casting formation preparation method in maynetostatic field
CN1453111A (en) * 2003-03-31 2003-11-05 浙江大学 Press filtering process to form functional gradient material in static magnetic field
CN1460661A (en) * 2003-06-03 2003-12-10 浙江大学 Method for preparing functional gradient material by adopting doctor-blade casting process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10258479A (en) * 1997-03-21 1998-09-29 Honda Motor Co Ltd Manufacture of functionally gradient material
US6248286B1 (en) * 1999-12-03 2001-06-19 Ut-Battelle, Llc Method of making a functionally graded material
CN1438084A (en) * 2003-02-21 2003-08-27 浙江大学 Functional gradient material slip-casting formation preparation method in maynetostatic field
CN1453111A (en) * 2003-03-31 2003-11-05 浙江大学 Press filtering process to form functional gradient material in static magnetic field
CN1460661A (en) * 2003-06-03 2003-12-10 浙江大学 Method for preparing functional gradient material by adopting doctor-blade casting process

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Assignee: Zibo Luming High Temperature Material Science and Technology Co., Ltd.

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